CN102030528A - Dielectric ceramic material with high-temperature stability and preparation method thereof - Google Patents

Dielectric ceramic material with high-temperature stability and preparation method thereof Download PDF

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CN102030528A
CN102030528A CN2009101769918A CN200910176991A CN102030528A CN 102030528 A CN102030528 A CN 102030528A CN 2009101769918 A CN2009101769918 A CN 2009101769918A CN 200910176991 A CN200910176991 A CN 200910176991A CN 102030528 A CN102030528 A CN 102030528A
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CN102030528B (en
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吴纪梁
吴迪
居涌
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WUXI AOLONG ELECTRONIC CO Ltd
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Abstract

The invention belongs to the field of capacitor dielectric material preparation and relates to a dielectric ceramic material with high-temperature stability and a preparation method thereof. The preparation method comprises the following steps of: pre-synthesizing base materials including barium titanate (BaTiO3), strontium titanate (SrTiO3), lead titanate (PbTiO3), calcium zirconate (CaZrO3) and Bi2O3.nTiO2 by using barium carbonate (BaCO3), strontium carbonate (SrCO3), calcium carbonate (CaCO3), lead oxide (PbO), bismuth trioxide (Bi2O3), zirconium oxide (ZrO2) and titanium oxide (TiO2) as raw materials and by a solid-phase synthesis process, wherein n is 1 to 5; according to a proportioning requirement, mixing the base materials and auxiliary additives including magnesium oxide (MgO) and manganese carbonate (MnCO3) and performing resynthesis by the solid-phase synthesis process; and then preparing the dielectric ceramic material with high-temperature stability by the preparation process of the conventional dielectric ceramic material. According to detection, a ceramic capacitor manufactured by the dielectric ceramic material has the electrical characteristics that: the temperature change rate, namely absolute value of delta epsilon/epsilon25, is less than or equal to 5 percent (between 25 DEG C below zero and 85 DEG C); the dielectric constant epsilon25 is more than or equal to 1,000; the tangent tg delta of a loss angle is less than or equal to 1 percent; and the breakdown voltage VBDC is more than or equal to 10 kV/mm.

Description

Dielectric ceramic material of a kind of high-temperature stability and preparation method thereof
Technical field
The present invention relates to the dielectric ceramic material technical field, particularly, relate to dielectric ceramic material of a kind of high-temperature stability and preparation method thereof.
Background technology
In today of electronic technology fast development, passive device day by day towards miniaturization, multifunction, high reliability and cheaply direction develop.Yet the quality base of all passive devices is all nothing more than the quality level of its corresponding function porcelain and the quality control degree in the manufacture craft, hereat makes the primary goal that to have high-quality function porcelain be all passive device manufacturing firms.
As the basis of hyundai electronics industry, as the important and main branch of passive device, advantage such as ceramic dielectric capacitor is little with its volume, specific volume is big, internal inductance is little and high frequency stability is good is at electrical condenser industry dominate all the time.Dielectric ceramic material is the basis of preparation ceramic condenser, and simultaneously it also has the characteristics of easily synthetic, low cost and suitable for industrial for it.
At present, with BaTiO 3Or has an ABO 3The perovskite structure starting material are the dielectric ceramic of principal crystalline phase preparation, often can not take into account specific inductivity and rate of temperature change thereof, loss tangent and to the dependency of voltage, also exist ceramic body fragility big simultaneously, are difficult to the shortcoming of mechanical workout; This has just proposed how to take into account the requirement of every performance of dielectric ceramic.
Along with developing rapidly of high-power component and precision wave filtering device, the temperature stability of dielectric ceramic is required to improve constantly; Simultaneously, since also diversified day by day to the requirement of dielectric ceramic body profile and configuration aspects, the dielectric ceramic temperature stability therefore improved, reduce porcelain body fragility and become particularly important.
Owing to have higher dielectric constant, BaTiO 3The system dielectric ceramic is considered to the pillar of electronic industry, but its specific inductivity has than major mutation near Curie temperature, and bigger with the variation of envrionment temperature.At present, the temperature stability (± 15%) that is widely used in the X7R dielectric ceramic of aspects such as mobile communication product, notebook computer, instrument can not satisfy the service requirements that laminated ceramic capacitor (MLCC) and current field disturb (EMI) wave filter.Therefore the dielectric temperature stability of improving dielectric ceramic is one of present research focus, and the current research that improves the dielectric ceramic temperature stability, mainly concentrates on prescription and preparation technology aspect based on the dielectric ceramic material of barium carbonate powder.
Summary of the invention
The objective of the invention is to: a kind of high-temperature stability dielectric ceramic material and preparation method thereof is provided.
This dielectric ceramic material possesses following electric property: rate of temperature change after processing condition are prepared into dielectric ceramic according to the rules | Δ ε | and/ε 25≤ 5% (25 ℃～85 ℃), DIELECTRIC CONSTANT 25〉=1000, loss tangent tg δ≤1%, voltage breakdown VB DC〉=10KV/mm.
For achieving the above object, according to an aspect of the present invention, provide a kind of dielectric ceramic material of high-temperature stability, comprised following basic material by percentage to the quality: BaTiO 3: 30～60wt%, SrTiO 3: 5～35wt%, PbTiO 3: 2～25wt%, CaZrO 3: 1～20wt%, Bi 2O 3NTiO 2: 1～30wt%; Based on above-mentioned basic material, also comprise additive by percentage to the quality: MgO:1～30wt%, MnCO 3: 0.01～1wt%; Described basic material BaTiO 3, SrTiO 3, PbTiO 3, CaZrO 3And Bi 2O 3NTiO 2All be by solid-phase synthesis synthetic material, described n=1～5.
For achieving the above object, according to another aspect of the present invention, provide a kind of preparation method of high-temperature stability dielectric ceramic material, comprised process for solid phase synthesis twice, be specially:
(1) solid-phase synthesis synthesizes base mateiral in advance for the first time
With BaCO 3, SrCO 3, CaCO 3, PbO, Bi 2O 3, ZrO 2And TiO 2As starting material, by the pre-respectively synthetic base mateiral BaTiO of solid-phase synthesis 3, SrTiO 3, PbTiO 3, Bi 2O 3NTiO 2And CaZrO 3
Pre-synthetic synthesis condition is: temperature rise rate: 100～300 ℃/hour, and soaking time: 1～5 hour, rate of temperature fall: 150～300 ℃/hour; BaTiO wherein 3, SrTiO 3And CaZrO 3Synthesis temperature be 1050～1300 ℃, PbTiO 3And Bi 2O 3NTiO 2Synthesis temperature be 600～900 ℃;
(2) dielectric ceramic material of solid-phase synthesis resynthesis high-temperature stability for the second time
Pre-synthetic base mateiral in the described step (1) is aided with additive MgO and MnCO 3, according to the proportioning described in the claim 1, carry out resynthesis, and then the dielectric ceramic material preparation technology who is aided with routines such as centrifugal granulating is prepared into the dielectric ceramic material of high-temperature stability by solid-phase synthesis;
The synthesis condition of resynthesis is: temperature rise rate: 100～300 ℃/hour, and synthesis temperature: 1050～1300 ℃, soaking time: 1～5 hour, rate of temperature fall: 150～300 ℃/hour.
Further, through twice process for solid phase synthesis and be aided with the dielectric ceramic material that the technology of routines such as centrifugal granulating is made, handle through 3000～30000 Gauss's deironing again, can be made into the dielectric ceramic material of high-temperature stability.
In above-mentioned preparation method, twice process for solid phase synthesis directly influences the over-all properties and the sintering temperature thereof of this dielectric ceramic material (after making ceramic condenser).
Further, the material behind the described resynthesis is handled through carrying out deironing behind the centrifugal granulating, and this deferrization process can directly influence the breakdown voltage property of dielectric ceramic material (after making ceramic condenser).
Will be through twice solid phase synthesis dielectric ceramic material behind the deferrization process, become the dielectric ceramic body and detect according to following processes:
(A) dry-pressing formed: compact density=3.0～4.0g/cm 3
(B) sintering:
Room temperature → 250 ℃/hour ↑ → 800 ℃ * 1 hour → 250 ℃/hour ↑ → 1250 ℃～1400 * 1～3 hours → 200 ℃/hour ↓ → 800 ℃ → 250 ℃/hour ↓ below → 200 ℃.
(C) preparation electrode: use the silver slurry of silver content 70wt%, silk screen printing, 10～20 minutes burning infiltration silver electrodes of 820 ℃ of insulations.
After testing, the dielectric ceramic electrical condenser that is processed into by this dielectric ceramic material possesses following electric property: rate of temperature change | Δ ε | and/ε 25≤ 5% (25 ℃～85 ℃), DIELECTRIC CONSTANT 25〉=1000, loss tangent tg δ≤1%, voltage breakdown VB DC〉=10KV/mm.
With respect to prior art, the present invention has following beneficial effect:
1, the basic material of the present invention's employing is through solid-phase synthesis synthetic titanate material, with respect to by chemical synthesis synthetic titanate material, helps the temperature stability of dielectric ceramic material.
2, the present invention adopts twice process for solid phase synthesis to synthesize dielectric ceramic material, compares with traditional sintering process, and the dielectric ceramic body that is processed into through this dielectric ceramic material possesses following electric property characteristics: the material temperature velocity of variation | Δ ε | and/ε 25≤ 5% (25 ℃～85 ℃), DIELECTRIC CONSTANT 25〉=1000, loss tangent tg δ≤1%, voltage breakdown VB DC〉=10KV/mm; Promptly, have excellent dielectric temperature stability and workability, can be used for the strict high voltage capacitor of temperature stability is reached the manufacturing of relevant components and parts having high dielectric constant and low-loss while.
3, adopt the prepared dielectric ceramic electrical condenser porcelain base of dielectric ceramic material of the present invention in mechanical processing process such as normal grinding, cutting, porcelain, cracked phenomenon can not occur collapsing.
4, cheap, the wide material sources of the selected cost of material of the present invention, the high-temperature stability of new prescription has good market outlook, can be used as the regeneration product of same type of material.
Embodiment
Embodiment 1
The dielectric ceramic material of high-temperature stability of the present invention is prepared as follows:
(1) selected starting material, its main content is greater than 98.5%.
(2) calculate the base mateiral prescription according to following mole proportioning:
BaCO 3: TiO 2=1: 1, be used to prepare BaTiO 3
SrCO 3: TiO 2=1: 1, be used to prepare SrTiO 3
PbO: TiO 2=1: 1, be used to prepare PbTiO 3
Bi 2O 3: nTiO 2=1: n is used to prepare Bi 2O 3NTiO 2(n=1～5);
CaCO 3: ZrO 2=1: 1, be used to prepare CaZrO 3
(3) will process according to following processing requirement according to calculating the also starting material of load weighted base mateiral in the step (2):
(A) wet ball-milling: ball milling time=12 hour.
(B) discharging and filter-press dehydration.
(C) drying: 120 ℃ kept 12 hours.
(D) briquetting: pressed density=2.2g/cm 3
(E) pre-synthetic: temperature rise rate=150 ℃/hour, BaTiO 3, SrTiO 3And CaZrO 3Synthesis temperature be 1200 ℃, PbTiO 3And Bi 2O 3NTiO 2Synthesis temperature be 750 ℃, soaking time=3 hour, rate of temperature fall=250 ℃/hour.
(F) fragmentation: the material granule degree after the rolling is less than 2mm.
(4) base mateiral that (3) step is produced calculates the proportioning of dielectric ceramic material involved in the present invention according to table 1:
The proportioning of table 1 dielectric ceramic material
Figure B2009101769918D0000051
(5) process according to calculating of (4) step and load weighted material according to following processing requirement:
(A) wet ball-milling: ball milling time=12h.
(B) discharging and filter-press dehydration.
(C) drying: 120 ℃ keep 12h.
(D) briquetting: pressed density=2.2g/cm 3
(E) resynthesis: temperature rise rate=150 ℃/h, synthesis temperature is 1150 ℃, soaking time=3h, rate of temperature fall=250 ℃/h.
(F) fragmentation: the material granule degree after the rolling is less than 2mm.
(G) wet ball-milling: ball milling time=24h.
(H) discharging: the slurry that ball milling is good leaves in the container.
(I) slurry sedimentation: allow and leave in more than the slurry natural subsidence 24h in the container.
(J) slurry preparation: with PVA tackiness agent, plasticizer, dispersion agent, defoamer and deionized water, it is 45%～50% centrifugal granulating slurry that the sedimentation disposed slurry is mixed with solid content.
(K) centrifugal granulating: 200 orders～350 purpose particle total amounts are 95wt%;
(L) deironing: the porcelain that granulation is good drops in the magnetic separator de-ironing that magnetic induction density is 30000 Gausses and carries out deironing;
To become ceramic condenser according to following processes through the dielectric ceramic material that above-mentioned steps obtains and detect.
(A) dry-pressing formed: compact density/3.4g/cm 3
(B) sintering:
Room temperature → 250 ℃/hour ↑ → 800 ℃ * 1 hour → 250 ℃/hour ↑ → 1320 ℃ * 2 hours → 200 ℃/hour ↓ → 800 ℃ → 250 ℃/hour ↓ below → 200 ℃.
(C) preparation electrode: use the silver slurry of silver content 70wt%, silk screen printing, 10 minutes burning infiltration silver electrodes of 820 ℃ of insulations.
After testing, the dielectric ceramic electrical condenser of making through dielectric ceramic material of the present invention possesses the described technical characteristic of table 2.
The technical characteristic of table 2 embodiment 1
Figure B2009101769918D0000061
Figure B2009101769918D0000071
Embodiment 2
The dielectric ceramic material of high-temperature stability of the present invention is prepared as follows:
(1) selected starting material, its main content is greater than 98.5%.
(2) calculate the base mateiral prescription according to following mole proportioning:
BaCO 3: TiO 2=1: 1, be used to prepare BaTiO 3
SrCO 3: TiO 2=1: 1, be used to prepare SrTiO 3
PbO: TiO 2=1: 1, be used to prepare PbTiO 3
Bi 2O 3: nTiO 2=1: n is used to prepare Bi 2O 3NTiO 2(n=1～5);
CaCO 3: ZrO 2=1: 1, be used to prepare CaZrO 3
(3) will process according to following processing requirement according to calculating the also starting material of load weighted base mateiral in the step (2):
(A) wet ball-milling: ball milling time=12 hour.
(B) discharging and filter-press dehydration.
(C) drying: 120 ℃ kept 12 hours.
(D) briquetting: pressed density=2.2g/cm 3
(E) pre-synthetic: temperature rise rate=150 ℃/hour, BaTiO 3, SrTiO 3And CaZrO 3Synthesis temperature be 1200 ℃, PbTiO 3And Bi 2O 3NTiO 2Synthesis temperature be 750 ℃, soaking time=3 hour, rate of temperature fall=250 ℃/hour.
(F) fragmentation: the material granule degree after the rolling is less than 2mm.
(4) base mateiral that (3) step is produced calculates the proportioning of dielectric ceramic material involved in the present invention according to table 3:
The proportioning of table 3 dielectric ceramic material
Figure B2009101769918D0000081
(5) process according to calculating of (4) step and load weighted material according to following processing requirement:
(A) wet ball-milling: ball milling time=12h.
(B) discharging and filter-press dehydration.
(C) drying: 120 ℃ keep 12h.
(D) briquetting: pressed density=2.2g/cm 3
(E) resynthesis: synthetic and 1150 ℃ of resynthesis compare.
(F) fragmentation: the material granule degree after the rolling is less than 2mm.
(G) wet ball-milling: ball milling time=24h.
(H) discharging: the slurry that ball milling is good leaves in the container.
(I) slurry sedimentation: allow and leave in more than the slurry natural subsidence 24h in the container.
(J) slurry preparation: with PVA tackiness agent, plasticizer, dispersion agent, defoamer and deionized water, it is 45%～50% centrifugal granulating slurry that the sedimentation disposed slurry is mixed with solid content.
(K) centrifugal granulating: 200 orders～350 purpose particle total amounts are 95wt%;
(L) deironing: the porcelain that granulation is good drops in the magnetic separator de-ironing that magnetic induction density is 30000 Gausses and carries out deironing.
To become ceramic condenser according to following processes through the dielectric ceramic material that above-mentioned steps obtains and detect.
(A) dry-pressing formed: compact dimensions is Φ 10 * 1mm, compact density=3.4g/cm 3
(B) sintering:
Room temperature → 250 ℃/hour ↑ → 800 ℃ * 1 hour → 250 ℃/hour ↑ → 1320 ℃ * 2 hours → 200 ℃/hour ↓ → 800 ℃ → 250 ℃/hour ↓ below → 200 ℃.
(C) preparation electrode: use the silver slurry of silver content 70wt%, silk screen printing, 10 minutes burning infiltration silver electrodes of 820 ℃ of insulations.
After testing, the dielectric ceramic electrical condenser of making through dielectric ceramic material of the present invention possesses the described technical characteristic of table 4.
The technical characteristic of table 4 embodiment 2
Figure B2009101769918D0000091
Embodiment 3
The dielectric ceramic material of high-temperature stability of the present invention is prepared as follows:
(1) selected starting material, its main content is greater than 98.5%.
(2) calculate the base mateiral prescription according to following mole proportioning:
BaCO 3: TiO 2=1: 1, be used to prepare BaTiO 3
SrCO 3: TiO 2=1: 1, be used to prepare SrTiO 3
PbO: TiO 2=1: 1, be used to prepare PbTiO 3
Bi 2O 3: nTiO 2=1: n is used to prepare Bi 2O 3NTiO 2(n=1～5);
CaCO 3: ZrO 2=1: 1, be used to prepare CaZrO 3
(3) will process according to following processing requirement according to calculating the also starting material of load weighted base mateiral in the step (2):
(A) wet ball-milling: ball milling time=12 hour.
(B) discharging and filter-press dehydration.
(C) drying: 120 ℃ kept 12 hours.
(D) briquetting: pressed density=2.2g/cm 3
(E) pre-synthetic: temperature rise rate=100 ℃/hour, BaTiO 3, SrTiO 3And CaZrO 3Synthesis temperature be 1050 ℃, PbTiO 3And Bi 2O 3NTiO 2Synthesis temperature be 600 ℃, soaking time=5 hour, rate of temperature fall=150 ℃/hour.
(F) fragmentation: the material granule degree after the rolling is less than 2mm.
(4) base mateiral that (3) step is produced calculates the proportioning of dielectric ceramic material involved in the present invention according to table 5:
The proportioning of table 5 dielectric ceramic material
Figure B2009101769918D0000101
(5) process according to calculating of (4) step and load weighted material according to following processing requirement:
(A) wet ball-milling: ball milling time=12h.
(B) discharging and filter-press dehydration.
(C) drying: 120 ℃ keep 12h.
(D) briquetting: pressed density=2.2g/cm 3
(E) resynthesis: temperature rise rate=100 ℃/h, synthesis temperature is 1050 ℃, soaking time=5h, rate of temperature fall=150 ℃/h.
(F) fragmentation: the material granule degree after the rolling is less than 2mm.
(G) wet ball-milling: ball milling time=24h.
(H) discharging: the slurry that ball milling is good leaves in the container.
(I) slurry sedimentation: allow and leave in more than the slurry natural subsidence 24h in the container.
(J) slurry preparation: with PVA tackiness agent, plasticizer, dispersion agent, defoamer and deionized water, it is 45%～50% centrifugal granulating slurry that the sedimentation disposed slurry is mixed with solid content.
(K) centrifugal granulating: 200 orders～350 purpose particle total amounts are 95wt%;
(L) deironing: the porcelain that granulation is good drops in the magnetic separator de-ironing that magnetic induction density is 3000 Gausses and carries out deironing.
(M) dry-pressing formed: compact dimensions is Φ 10 * 1mm, compact density=3.0g/cm 3
(N) sintering:
Room temperature → 250 ℃/hour ↑ → 800 ℃ * 1 hour → 250 ℃/hour ↑ → 1250 ℃ * 3 hours → 200 ℃/hour ↓ → 800 ℃ → 250 ℃/hour ↓ below → 200 ℃.
(O) preparation electrode: use the silver slurry of silver content 70wt%, silk screen printing, 10 minutes burning infiltration silver electrodes of 820 ℃ of insulations.
Embodiment 4
The dielectric ceramic material of high-temperature stability of the present invention is prepared as follows:
(1) selected starting material, its main content is greater than 98.5%.
(2) calculate the base mateiral prescription according to following mole proportioning:
BaCO 3: TiO 2=1: 1, be used to prepare BaTiO 3
SrCO 3: TiO 2=1: 1, be used to prepare SrTiO 3
PbO: TiO 2=1: 1, be used to prepare PbTiO 3
Bi 2O 3: nTiO 2=1: n is used to prepare Bi 2O 3NTiO 2(n=1～5);
CaCO 3: ZrO 2=1: 1, be used to prepare CaZrO 3
(3) will process according to following processing requirement according to calculating the also starting material of load weighted base mateiral in the step (2):
(A) wet ball-milling: ball milling time=12 hour.
(B) discharging and filter-press dehydration.
(C) drying: 120 ℃ kept 12 hours.
(D) briquetting: pressed density=2.2g/cm 3
(E) pre-synthetic: temperature rise rate=300 ℃/hour, BaTiO 3, SrTiO 3And CaZrO 3Synthesis temperature be 1300 ℃, PbTiO 3And Bi 2O 3NTiO 2Synthesis temperature be 900 ℃, soaking time=1 hour, rate of temperature fall=300 ℃/hour.
(F) fragmentation: the material granule degree after the rolling is less than 2mm.
(4) base mateiral that (3) step is produced calculates the proportioning of dielectric ceramic material involved in the present invention according to table 5:
The proportioning of table 6 dielectric ceramic material
Figure B2009101769918D0000121
(5) process according to calculating of (4) step and load weighted material according to following processing requirement:
(A) wet ball-milling: ball milling time=12h.
(B) discharging and filter-press dehydration.
(C) drying: 120 ℃ keep 12h.
(D) briquetting: pressed density=2.2g/cm 3
(E) resynthesis: temperature rise rate=300 ℃/h, synthesis temperature is 1300 ℃, soaking time=1h, rate of temperature fall=300 ℃/h.
(F) fragmentation: the material granule degree after the rolling is less than 2mm.
(G) wet ball-milling: ball milling time=24h.
(H) discharging: the slurry that ball milling is good leaves in the container.
(I) slurry sedimentation: allow and leave in more than the slurry natural subsidence 24h in the container.
(J) slurry preparation: with PVA tackiness agent, plasticizer, dispersion agent, defoamer and deionized water, it is 45%～50% centrifugal granulating slurry that the sedimentation disposed slurry is mixed with solid content.
(K) centrifugal granulating: 200 orders～350 purpose particle total amounts are 95wt%;
(L) deironing: the porcelain that granulation is good drops in the magnetic separator de-ironing that magnetic induction density is 30000 Gausses and carries out deironing.
(M) dry-pressing formed: compact dimensions is Φ 10 * 1mm, compact density=4.0g/cm 3
(N) sintering:
Room temperature → 250 ℃/hour ↑ → 800 ℃ * 1 hour → 250 ℃/hour ↑ → 1400 ℃ * 1 hour → 200 ℃/hour ↓ → 800 ℃ → 250 ℃/hour ↓ below → 200 ℃.
(O) preparation electrode: use the silver slurry of silver content 70wt%, silk screen printing, 10 minutes burning infiltration silver electrodes of 820 ℃ of insulations.
After testing, the dielectric ceramic electrical condenser of making through dielectric ceramic material of the present invention has following electrical specification: rate of temperature change | Δ ε | and/ε 25≤ 5% (25 ℃～85 ℃), DIELECTRIC CONSTANT 25〉=1000, loss tangent tg δ≤1%, voltage breakdown VB DC〉=10KV/mm.

Claims (3)

1. the dielectric ceramic material of a high-temperature stability is characterized in that, comprises following basic material by percentage to the quality: BaTiO 3: 30～60wt%, SrTiO 3: 5～35wt%, PbTiO 3: 2～25wt%, CaZrO 3: 1～20wt%, Bi 2O 3NTiO 2: 1～30wt%;
Based on above-mentioned basic material, also comprise additive by percentage to the quality: MgO:1～30wt%, MnCO 3: 0.01～1wt%;
Described basic material BaTiO 3, SrTiO 3, PbTiO 3, CaZrO 3And Bi 2O 3NTiO 2All be by solid-phase synthesis synthetic material, described n=1～5.
2. the preparation method of the dielectric ceramic material of a kind of high-temperature stability according to claim 1 is characterized in that, comprises process for solid phase synthesis twice, is specially:
(1) solid-phase synthesis synthesizes base mateiral in advance for the first time
With BaCO 3, SrCO 3, CaCO 3, PbO, Bi 2O 3, ZrO 2And TiO 2As starting material, by the pre-respectively synthetic base mateiral BaTiO of solid-phase synthesis 3, SrTiO 3, PbTiO 3, Bi 2O 3NTiO 2And CaZrO 3
Pre-synthetic synthesis condition is: temperature rise rate: 100～300 ℃/hour, and soaking time: 1～5 hour, rate of temperature fall: 150～300 ℃/hour; BaTiO wherein 3, SrTiO 3And CaZrO 3Synthesis temperature be 1050～1300 ℃, PbTiO 3And Bi 2O 3NTiO 2Synthesis temperature be 600～900 ℃;
(2) dielectric ceramic material of solid-phase synthesis resynthesis high-temperature stability for the second time
Pre-synthetic base mateiral in the described step (1) is aided with additive MgO and MnCO 3, according to the proportioning described in the claim 1, carry out resynthesis, and then the dielectric ceramic material preparation technology who is aided with routines such as centrifugal granulating is prepared into the dielectric ceramic material of high-temperature stability by solid-phase synthesis;
The synthesis condition of resynthesis is: temperature rise rate: 100～300 ℃/hour, and synthesis temperature: 1050～1300 ℃, soaking time: 1～5 hour, rate of temperature fall: 150～300 ℃/hour.
3. the preparation method of the dielectric ceramic material of a kind of high-temperature stability according to claim 2, it is characterized in that, through twice process for solid phase synthesis and be aided with the technology of routines such as centrifugal granulating and the dielectric ceramic material made, handle through 3000～30000 Gauss's deironing again.
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CN105272232A (en) * 2015-10-12 2016-01-27 苏州法斯特信息科技有限公司 Barium titanate based composite capacitor ceramic material and preparation method thereof
CN105294101A (en) * 2014-06-03 2016-02-03 上海帛汉新材料科技有限公司 Dielectric material for high temperature stable type ceramic capacitor, and preparation method therefor and application thereof
CN107867826A (en) * 2017-11-23 2018-04-03 苏州科茂电子材料科技有限公司 A kind of preparation method of refractory ceramics dielectric material
CN108074737A (en) * 2016-11-17 2018-05-25 昆山万盛电子有限公司 A kind of patch safety electric capacity chip material and preparation method
CN108569901A (en) * 2017-03-07 2018-09-25 安徽升鸿电子有限公司 A kind of high-temperature dielectric material and preparation method thereof
CN109133915A (en) * 2018-08-30 2019-01-04 武汉理工大学 A kind of high energy storage barium phthalate base dielectric material and preparation method thereof

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CN108074737A (en) * 2016-11-17 2018-05-25 昆山万盛电子有限公司 A kind of patch safety electric capacity chip material and preparation method
CN108569901A (en) * 2017-03-07 2018-09-25 安徽升鸿电子有限公司 A kind of high-temperature dielectric material and preparation method thereof
CN107867826A (en) * 2017-11-23 2018-04-03 苏州科茂电子材料科技有限公司 A kind of preparation method of refractory ceramics dielectric material
CN109133915A (en) * 2018-08-30 2019-01-04 武汉理工大学 A kind of high energy storage barium phthalate base dielectric material and preparation method thereof
CN109133915B (en) * 2018-08-30 2021-11-16 武汉理工大学 Barium titanate-based dielectric material with high energy storage capacity and preparation method thereof

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